The extraction of metal diethyldithiocarbamate complexes into chloroform from an alkaline solution containing cyanide and citrate ions is a convenient means of separating small amounts of bismuth and lead from copper and uranium, and from the elements normally found in copper-base alloys. After the separation, bismuth and lead are determined polarographically using an acidic tartrate solution as the supporting electrolyte.The method is applicable to the determination of bismuth and lead, in the concentration range from 0.0005–0.05%, in copper-base alloys of widely different composition.